CN104055838A - Extraction method of walnut green seedcase polyphenol - Google Patents
Extraction method of walnut green seedcase polyphenol Download PDFInfo
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Abstract
The invention discloses an extraction method of walnut green seedcase polyphenol, which comprises the following steps: selecting fresh walnuts as raw materials, mechanically peeling to obtain walnut green seedcases, blanching, then naturally drying in the sun, pulverizing, and passing through a 40-mesh screen; and adding pure water into the dried, pulverized and screened walnut green seedcases according to a liquid-solid ratio of 21:1(mL:g), putting in ultrasonic wave extraction equipment, and performing an ultrasonic wave aided extraction process, wherein the ultrasonic power is 670W, the heating temperature is 57 DEG C, the single ultrasonic time is 5s, the ultrasonic interval time is 5s, the full ultrasonic time is 25 minutes, and the stirring speed is 400 r/min. The polyphenol yield can be up to 55.473 mg/g. The extraction method disclosed by the invention has favorable application prospects in walnut green seedcase polyphenol production.
Description
Technical field
The present invention relates to fruit polyphenol and extract preparing technical field, specifically, the present invention relates to a kind of preparation technology's who extracts polyphenol from Exocarpium Juglandis Immaturus technical field.
Background technology
Semen Juglandis is the perennial deciduous tree of Juglandaceae Juglans, and in China, it is mainly distributed in the provinces such as Xinjiang, Yunnan, Hebei, Shandong.Exocarpium Juglandis Immaturus, has another name called Exocarpium Juglandis Immaturum, is the immature epicarp of Semen Juglandis.Modern study shows, Exocarpium Juglandis Immaturus contains abundant polyphenols, has antitumor, antioxidation, antiviral, antibacterial isoreactivity.
2,800,000 mu of Xinjiang Semen Juglandis cultivated areas, produce 240000 tons of dry fruit Semen Juglandiss per year, Exocarpium Juglandis Immaturus annual production is 360,000 tons of left and right, owing to further not carrying out processing and utilization, a large amount of discarded Pericarpium Citri Reticulatae Virides are deposited in field, the edge of a field or limes marginis, not only can cause the significant wastage of resource, also can serious pollution of ecological environment, jeopardize vegeto-animal existence.In the application of Juglans plants polyphenols research, be still in the junior stage at present, therefore study and extract polyphenol Technology taking Exocarpium Juglandis Immaturus as raw material, development to Walnut Industry chain, realize garbage and just fully utilize significant.
Summary of the invention
Have no about the state of the art for extracting polyphenol in Exocarpium Juglandis Immaturus for existing, the present invention aims to provide a kind of extracting method of Exocarpium Juglandis Immaturus polyphenol, the present invention is around the technical problem of a large amount of Exocarpium Juglandis Immaturus comprehensive utilizations that produce in Semen Juglandis production process, obtain the production technology that Exocarpium Juglandis Immaturus polyphenol substance extracts, for suitability for industrialized production Exocarpium Juglandis Immaturus polyphenol substance provides technical support, to solve the problem of complex utilization in the Walnut Industry Development of Xinjiang, to lengthening manufacturing chain, promote intensive processing and the level of comprehensive utilization of Semen Juglandis, the added value aspect that improves Semen Juglandis processed goods all has great importance and is worth.
The present invention is achieved through the following technical solutions.
The present invention taking through the dry Exocarpium Juglandis Immaturus of pretreatment as raw material, utilize the process conditions of response surface method Optimization for Ultrasonic Wave assisted extraction polyphenol, by by Exocarpium Juglandis Immaturus blanching, naturally dry, pulverize, mix with pure water and be placed in ultrasonic extraction equipment and extract under different technology conditions, on the basis of single factor experiment, select the comparatively significant ultrasonic power of polyphenol yield impact, heating-up temperature, three factors of liquid ratio are independent variable, taking polyphenol yield as response value, carry out Box-behnken test and response surface analysis, show that optimum process condition is: ultrasonic power 670W, 57 DEG C of heating-up temperatures, liquid ratio 21:1 (mL:g), single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 25min, mixing speed 400r/min, under the process conditions that obtain, polyphenol yield can be up to 55.473mg/g, technological parameter is workable, can be for the extraction of Exocarpium Juglandis Immaturus polyphenol substance.
The present invention specifically provides a kind of extracting method of Exocarpium Juglandis Immaturus polyphenol, and concrete extracting method is as follows:
Choosing fresh Semen Juglandis is raw material, adopt machine barking method to obtain Exocarpium Juglandis Immaturus, through blanching, naturally pulverized 40 mesh sieves after drying, Exocarpium Juglandis Immaturus powder after drying is pulverized and sieved adds pure water by liquid ratio 21:1 (mL:g), be placed in ultrasonic extraction equipment, adopt ultrasound wave assisted extraction Exocarpium Juglandis Immaturus polyphenol, technological parameter is ultrasonic power 670W, 57 DEG C of heating-up temperatures,, single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 25min, mixing speed 400r/min.
The pretreatment of the Exocarpium Juglandis Immaturus that the present invention adopts, although the technological means such as ultrasound wave assisted extraction be unable to do without support and the inspiration of prior art, but for the extraction of polyphenol, particularly for the extraction for polyphenol in Exocarpium Juglandis Immaturus raw material, for the storage rate that improves polyphenol in Exocarpium Juglandis Immaturus adopts hot air drying, naturally dry, 65 DEG C of hot air dryings after blanching, the different dry-making method of dried of multiple Exocarpium Juglandis Immaturus such as after blanching, naturally dry, select to be applicable to the suitable ultrasound wave assisted extraction technique that Exocarpium Juglandis Immaturus polyphenol extracts, for the height of extraction ratio that determines polyphenol, the efficiency of extracting all has important effect, also be deciding factor, the technological means of talkative employing and instrument are not prior aries, and then negate the novelty of the extracting method of overall Exocarpium Juglandis Immaturus polyphenol provided by the invention, existing all technological inventions and innovation be unable to do without support and the basis of prior art.Visible, in the extracting method of Exocarpium Juglandis Immaturus polyphenol provided by the invention, each technical factor and technical parameter all pass through comprehensive consideration and design, in the extracting method of Exocarpium Juglandis Immaturus polyphenol provided by the invention, each sport technique segment has upper and lower one, any technical step is indispensable, tight indivisible feature, can not any choice dismember technical step wherein.
Object of the present invention is around the technical problem of a large amount of Exocarpium Juglandis Immaturus comprehensive utilizations that produce in Semen Juglandis production process, obtain the processing parameter that Exocarpium Juglandis Immaturus polyphenol substance extracts, adopt the oxidation of Exocarpium Juglandis Immaturus being carried out blanching processing and prevented with passive oxidation enzymatic activity polyphenol substance, the preprocess method that improves Exocarpium Juglandis Immaturus polyphenol storage rate improves the content of polyphenol in Exocarpium Juglandis Immaturus greatly, ultrasound wave assisted extraction technique used in the present invention, be energy gathering type and divergence expression ultrasound wave are combined and Circulation in material, it is energy gathering type, divergence expression ultrasonic field stationary distribution, under stirring action, make Matter Transfer pass through successively ultrasonic field, thereby improve to greatest extent the utilization rate of ultrasonic field, solve static material limited problem of sphere of action in the time of supersound extraction, increase the material treating capacity of ultrasonic field, improve efficiency.Taking pure water as extracting when solvent extraction ratio up to 55.473mg/g, and there is the advantages such as with low cost, safe, pollution-free taking water as extracting solvent.
by implementing the concrete summary of the invention of the present invention, can reach following effect:
The present invention is by the technological parameter that Exocarpium Juglandis Immaturus is carried out to pretreatment, adopts ultrasound wave assisted extraction technique, carries out Box-behnken test and the extraction of response surface analysis optimization Exocarpium Juglandis Immaturus polyphenol taking polyphenol yield as response value, draw optimum process condition, under acquisition process conditions, polyphenol yield can be up to 55.473mg/g, and the method has good application prospect in Exocarpium Juglandis Immaturus polyphenol is produced.
Brief description of the drawings
Fig. 1 is shown as the affect figure of different dry-making method of dried on polyphenol storage rate.
Fig. 2 is shown as the affect figure of mixing speed on polyphenol yield.
Fig. 3 is shown as the affect figure of ultrasonic off time on polyphenol yield.
Fig. 4 is shown as the affect figure of ultrasonic omnidistance time on polyphenol yield.
Fig. 5 is shown as the affect figure of ultrasonic power on polyphenol yield.
Fig. 6 is shown as the affect figure of temperature on polyphenol yield.
Fig. 7 is shown as the affect figure of liquid ratio on polyphenol yield.
Fig. 8 is shown as the reciprocal action response surface chart of ultrasonic power and heating-up temperature.
Fig. 9 is shown as the reciprocal action response surface figure of ultrasonic power and liquid ratio.
Figure 10 is shown as the reciprocal action response surface figure of heating-up temperature and liquid ratio.
Detailed description of the invention
, for embodiment, the present invention is described below, still, the present invention is not limited to following embodiment.In addition, in the test of following each embodiment is described, without special instruction, % all refers to mass percent, by m/m.
Instrument and equipment: AL204-IC type electronic balance, Mettler-Toledo Instrument (Shanghai) Co., Ltd.; SB-2000 type digital control constant temperature water-bath, Shanghai Ai Lang Instrument Ltd.; TU-1810 ultraviolet-uisible spectrophotometer, Beijing Puxi General Instrument Co., Ltd; Anke LXJ-II B centrifuge, Anting Scientific Instrument Factory, Shanghai; CTXNW-2B ultrasonic circulating extractor, Beijing Hongxianglong Biotechnology Development Co., Ltd.
Raw material adopts Exocarpium Juglandis Immaturus to pluck from Wushi County, city of Aksu of Xinjiang, through blanching, naturally pack, keep in Dark Place after drying, pulverizes 40 mesh sieves when use; Reagent adopts gallic acid, natrium carbonicum calcinatum, and sodium tungstate, sodium molybdate, lithium sulfate, bromine water, strong phosphoric acid, concentrated hydrochloric acid, is analytical pure.
All reagent, instrument, the raw and auxiliary material in the present invention, selected are all well known selecting, but do not limit enforcement of the present invention, and other reagent more well known in the art and equipment are all applicable to the enforcement of the following embodiment of the present invention.
embodiment mono-: the extraction of Exocarpium Juglandis Immaturus polyphenol
The concrete grammar of the extraction of Exocarpium Juglandis Immaturus polyphenol is as follows.
(1) preparation of Exocarpium Juglandis Immaturus raw material: choosing fresh Semen Juglandis is raw material, adopt machine barking method to obtain Exocarpium Juglandis Immaturus, respectively through 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C hot air dryings, naturally dry, after 65 DEG C of hot air dryings, blanching, naturally dry after blanching 8 kinds of dry-making method of dried and keep in Dark Place after drying.Polyphenol content is measured: after dry Exocarpium Juglandis Immaturus is pulverized, cross 40 mesh sieves, adopt 30% ethanol, liquid ratio 25:1(mL/g), the condition of temperature 50 C, extraction time 1h of extracting is carried out the extraction of polyphenol and the mensuration of content, to investigate the impact of different dry-making method of dried on polyphenol storage rate.Result is: 8 kinds of dried polyphenol contents of dry-making method of dried order is from high to low: after blanching, after 65 DEG C of hot air drying ﹥ blanching, naturally dry 55 DEG C of hot air drying ﹥ of 60 DEG C of hot air drying ﹥ of 65 DEG C of hot air drying ﹥ of 45 DEG C of hot air drying ﹥ of ﹥ and naturally dry 50 DEG C of hot air dryings of ﹥, polyphenol content (85.03mg/g(butt) with fresh Exocarpium Juglandis Immaturus) compared with, its loss rate is respectively 34.25%, 34.32%, 37.61%, 38.06%, 39.07%, 40.39%, 42.9%, 43.12%.Simultaneously known after blanching the loss rate of 65 DEG C of hot air dryings polyphenol compared with naturally drying after blanching differ less; and hot air drying energy consumption is high; therefore the method that adopts nature to dry after blanching is energy-conservation and the best practice of suitability for scale production; so the method for naturally drying after selection blanching is dried Exocarpium Juglandis Immaturus, referring to accompanying drawing 1.
(2) the fixing liquid ratio 20:1(mL:g of Exocarpium Juglandis Immaturus powder after drying is pulverized) meter adds pure water, is placed in ultrasonic extraction equipment, adopts ultrasound wave assisted extraction technique to carry out the extraction of polyphenol substance.
(3) single factor experiment that Exocarpium Juglandis Immaturus polyphenol extracts: fixing single ultrasonic time 5s, investigates the impact of 6 factors such as mixing speed, ultrasonic off time, ultrasonic omnidistance time, ultrasonic power, heating-up temperature, liquid ratio on Exocarpium Juglandis Immaturus polyphenol yield.
It is 0r/min, 400r/min, 600r/min, 800r/min, 1200r/min, 1600r/min that mixing speed is set respectively, fixing liquid ratio 20:1(mL:g), ultrasonic power 600W, 60 DEG C of heating-up temperatures, single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 15min, investigates the impact of different mixing speeds on Exocarpium Juglandis Immaturus polyphenol yield.
By ultrasonic off time of 1s, 3s, 5s, 7s, 9s are set respectively, fixing liquid ratio 20:1(mL:g), ultrasonic power 600W, mixing speed 400r/min, 60 DEG C of heating-up temperatures, single ultrasonic time 5s, ultrasonic omnidistance time 15min, investigates the impact of different ultrasonic off times on Exocarpium Juglandis Immaturus polyphenol yield.
Be 10min, 15min, 20min, 25min, 30min by the ultrasonic omnidistance time is set respectively, fixing liquid ratio 20:1(mL:g), ultrasonic power 600W, mixing speed 400r/min, 60 DEG C of heating-up temperatures, single ultrasonic time 5s, ultrasonic off time, 5s, investigated the impact of different ultrasonic omnidistance time on Exocarpium Juglandis Immaturus polyphenol yield.
By ultrasonic power 200W, 400W, 600W, 800W, 1000W are set respectively, fixing liquid ratio 20:1(mL:g), mixing speed 400r/min, 60 DEG C of heating-up temperatures, single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 15min, investigates the impact of different ultrasonic powers on Exocarpium Juglandis Immaturus polyphenol yield.
By 40 DEG C of heating-up temperatures, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C are set respectively, fixing liquid ratio 20:1(mL:g), ultrasonic power 600W, mixing speed 400r/min, single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 15min, investigates the impact of different temperatures on Exocarpium Juglandis Immaturus polyphenol yield.
By adopting respectively liquid ratio 10:1,15:1,20:1,25:1,30:1(mL:g), 60 DEG C of heating-up temperatures, ultrasonic power 600W, mixing speed 400r/min, single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 15min, investigates the impact of different liquid ratios on Exocarpium Juglandis Immaturus polyphenol yield.
(4) response surface test: according to Box-Benhnken center combination EXPERIMENTAL DESIGN principle, select heating-up temperature, ultrasonic power, solid-liquid ratio affects significant three factors to Exocarpium Juglandis Immaturus polyphenol yield, on the basis of single factor experiment, carrying out response surface EXPERIMENTAL DESIGN is optimized the process conditions of ultrasound wave assisted extraction Exocarpium Juglandis Immaturus polyphenol, the optimal processing parameter that obtains ultrasound wave assisted extraction Exocarpium Juglandis Immaturus polyphenol is: ultrasonic power 670W, 57 DEG C of heating-up temperatures, liquid ratio 21:1 (mL:g), single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 25min, mixing speed 400r/min.
Therefore the extracting method of the Exocarpium Juglandis Immaturus polyphenol that the present invention adopts, is raw material by choosing fresh Semen Juglandis, adopt machine barking method to obtain Exocarpium Juglandis Immaturus, after blanching, adopt nature to dry, pulverize after cross 40 mesh sieves, the Exocarpium Juglandis Immaturus powder after drying is pulverized and sieved by
ratioadd pure water, be placed in ultrasonic extraction equipment, adopt ultrasound wave assisted extraction technique, ultrasonic power 670W, 57 DEG C of heating-up temperatures, liquid ratio 21:1 (mL:g), single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 25min, mixing speed 400r/min.
embodiment bis-: the single factor experiment that Exocarpium Juglandis Immaturus polyphenol extracts
Based on above-described embodiment, the extracting method of the Exocarpium Juglandis Immaturus polyphenol of employing, is raw material by choosing fresh Semen Juglandis, adopt machine barking method to obtain Exocarpium Juglandis Immaturus, after blanching, adopt nature to dry, pulverize after cross 40 mesh sieves, the Exocarpium Juglandis Immaturus powder after drying is pulverized and sieved by
ratioadd pure water, be placed in ultrasonic extraction equipment, through ultrasound wave assisted extraction technique, concrete technology Verification single factor experiment is as follows.
At fixing single ultrasonic time 5s, respectively with 0r/min, 400r/min, 600r/min, 800r/min, 1200r/min, the mixing speed that 1600r/min is different, with 200W, 400W, 600W, 800W, the ultrasonic power that 1000W is different, with 1s, 3s, 5s, 7s, the ultrasonic off time that 9s is different, with 10min, 15min, 20min, 25min, the ultrasonic omnidistance time that 30min is different, with 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C of different heating-up temperatures, with 10:1, 15:1, 20:1, 25:1, the factors such as the liquid ratio (mL:g) that 30:1 is different are carried out single factor experiment, to study the impact of different factors on Exocarpium Juglandis Immaturus polyphenol yield.
results and analysis:
The impact of 1.1 mixing speeds on polyphenol yield: known referring to accompanying drawing 2, polyphenol yield is up to 44.13mg/g in the time that mixing speed is 400r/min, therefore select 400r/min as best mixing speed.
The impact of 1.2 ultrasonic off times on polyphenol yield: known referring to accompanying drawing 3, polyphenol yield is along with the prolongation of ultrasonic off time is totally the rear downward trend that first rises, and polyphenol yield is up to 42.65mg/g in the time that be 5s ultrasonic off time.Therefore selecting best ultrasonic off time is 5s.
1.3 the impact of ultrasonic omnidistance time on polyphenol yield: known referring to accompanying drawing 4, polyphenol yield is up to 42.89mg/g in the time that the ultrasonic omnidistance time is 25min, declines on the contrary along with the continuation of time extends polyphenol yield, and this is likely due to part polyphenol oxidase.Therefore selecting the best ultrasonic omnidistance time is 25min.
The impact of 1.4 ultrasonic powers on polyphenol yield: known referring to accompanying drawing 5, polyphenol yield is totally with the rising of ultrasonic power the rear downward trend that first rises, and polyphenol yield is up to 48.73mg/g in the time that ultrasonic power is 600W.This is due to the increase along with ultrasonic power, and cavitation strengthens, and has accelerated the fragmentation of cell, thereby has improved the yield of polyphenol; But in the time that ultrasonic power exceedes 600W, may be the stripping that hinders polyphenol due to the stripping meeting of some macromolecular substances, can reduce on the contrary the yield of polyphenol.Therefore selecting best ultrasonic power is 600W.
The impact of 1.5 temperature on polyphenol yield: known referring to accompanying drawing 6, polyphenol yield increases with the rising of temperature, and increase trend is obvious between 50 DEG C～60 DEG C, along with the continuation of temperature raises, the increase of polyphenol yield is relatively slow, and the temperature required energy consumption that raises also can correspondingly increase.Considering selection optimum temperature is 60 DEG C, and now polyphenol yield is 43.93mg/g.
The impact of 1.6 liquid ratios on polyphenol yield: known referring to accompanying drawing 7, when liquid ratio is less than 20:1(mL:g) time, polyphenol yield increases with liquid ratio, but is greater than 20:1(mL:g when liquid ratio) time, polyphenol yield remains unchanged substantially.Therefore selecting best liquid ratio is 20:1(mL:g), now polyphenol yield is 42.52mg/g.
Conclusion: as fully visible, by analyzing in mixing speed, ultrasonic off time, ultrasonic omnidistance time, ultrasonic power, heating-up temperature, the multiple factors of liquid ratio different parameters, the variation tendency of polyphenol yield impact is thought to ultrasonic power, heating-up temperature, three factors of liquid ratio are comparatively remarkable on the impact of polyphenol yield, therefore in follow-up test, fix single ultrasonic time 5s, the further reciprocal action between research ultrasonic power, heating-up temperature, three factors of liquid ratio after ultrasonic off time 5s, ultrasonic omnidistance time 25min, mixing speed 400r/min
,to obtain the optimal processing parameter of ultrasound wave assisted extraction Exocarpium Juglandis Immaturus polyphenol.
embodiment tri-: the response surface test of Exocarpium Juglandis Immaturus polyphenol
Known by above-described embodiment two single factor experiments, ultrasonic power, heating-up temperature, three factors of liquid ratio affect comparatively remarkable on polyphenol yield.Therefore select ultrasonic power, heating-up temperature, three factors of liquid ratio, carry out Box-behnken test taking polyphenol yield as response value, be shown in Table 1, utilize Design Expert8.0.5.b software to carry out data analysis, with the technological parameter of Optimization for Ultrasonic Wave assisted extraction Exocarpium Juglandis Immaturus polyphenol.
Table 1 response surface factor level coding schedule
The interpretation of result of 1.1 response surfaces:
Table 2 Box-benhnken experimental design result
The variance analysis of table 3 response surface secondary model
| Soruces of variation | Quadratic sum | Degree of freedom | Mean square | F value | P value | Significance |
| Model | 674.16 | 9 | 74.91 | 45.78 | ＜0.0001 | ** |
| A | 42.49 | 1 | 42.49 | 25.96 | 0.0014 | ** |
| B | 157.30 | 1 | 157.30 | 96.13 | ＜0.0001 | ** |
| C | 8.16 | 1 | 8．16 | 4.99 | 0.0607 | |
| AB | 6.99 | 1 | 6.99 | 4.27 | 0.0776 | |
| AC | 0.071 | 1 | 0.071 | 0.044 | 0.8407 | |
| BC | 10.49 | 1 | 10.49 | 6.41 | 0.0391 | * |
| A 2 | 66.25 | 1 | 66.25 | 40.49 | 0.0004 | ** |
| B 2 | 309.75 | 1 | 309.75 | 189.3 | ＜0.0001 | ** |
| C 2 | 36.77 | 1 | 36.77 | 22.47 | 0.0021 | ** |
| Residual error | 11.45 | 7 | 1.64 | |||
| Lose intend to | 0.35 | 3 | 0.12 | 0.042 | 0.9868 | |
| Pure error | 11.10 | 4 | 2.78 | |||
| Summation | 685.61 | 16 |
Note: * * represents extremely remarkable; * represent significantly
By regression analysis, obtain the ternary quadratic regression equation of polyphenol yield:
Y=54.82 +2.30 A－4.43 B+1.01 C－1.32 AB +0.13AC－1.62BC－3.97 A
2－8.58 B
2－2.96 C
2
As shown in Table 3, regression model is extremely remarkable, the coefficient R of model
2=0.9833.Lose plan item not remarkable, illustrate that the degree of fitting of this regression equation and experiment is higher.Wherein, A, B, A
2, B
2, C
2extremely remarkable, BC is remarkable.Hence one can see that, and each factor is not to be simple linear relationship on the impact of polyphenol yield, between them, be have interactive.The interactive impact of each factor referring to accompanying drawing 8 to accompanying drawing 10, can be found out intuitively by accompanying drawing 8 to accompanying drawing 10, each factor to the size order of polyphenol yield influence degree is: B > A > C, that is: heating-up temperature > ultrasonic power > liquid ratio.
Determining of 1.2 optimum extraction conditions
Within the scope of each factor of choosing, utilize Design Expert8.0.5.b software to analyze, the optimum process condition that draws ultrasound wave assisted extraction Exocarpium Juglandis Immaturus polyphenol is: ultrasonic power 669.34W, 56.91 DEG C of heating-up temperatures, liquid ratio 21.32:1 (mL:g); With this understanding, the theoretical value of polyphenol yield is 56.039mg/g.For the reliability of inspection acquired results, adopt above-mentioned optimal conditions to carry out the extraction of polyphenol, consider probability and the convenience of practical operation, by adjustment of technology be: ultrasonic power 670W, 57 DEG C of heating-up temperatures, liquid ratio 21:1 (mL:g), the actual polyphenol yield that records is 55.473mg/g, very approaching with predictive value, illustrate that this model and practical situation are more identical, there is good operability.
Conclusion: by mixing speed, ultrasonic off time, ultrasonic omnidistance time, ultrasonic power, heating-up temperature, that liquid ratio is carried out single factor experiment is known, heating-up temperature, ultrasonic power, three factors of liquid ratio are comparatively obvious on the impact of polyphenol yield.Carry out response surface test therefore select these three factors, utilize Design Expert software to carrying out data analysis, the optimum process condition that draws ultrasound wave assisted extraction Exocarpium Juglandis Immaturus polyphenol is: ultrasonic power 670W, 57 DEG C of heating-up temperatures, liquid ratio 21:1 (mL:g), single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 25min, mixing speed 400r/min.With this understanding, the theoretical value of polyphenol yield is 56.039mg/g, the actual polyphenol yield that records of demonstration test is 55.473mg/g, has greatly improved polyphenol yield compared with single factor experiment, and therefore the technological parameter of ultrasound wave assisted extraction Exocarpium Juglandis Immaturus polyphenol has been optimized in response surface test effectively.
embodiment tetra-: the drafting of polyphenol standard curve
Accurately take 0.2500g gallic acid, after dissolving with distilled water, standardize solution is to 1000mL.Accurately pipette respectively again 1.0,2.0,3.0,4.0,5.0,6.0,7.0mL in 25mL volumetric flask, use distilled water standardize solution.Its concentration is respectively 10,20,30,40,50,60,70ug/mL.Then each Concentraton gradient accurately pipettes 1mL to color-comparison tube, more each color comparison tube adds respectively 1mLFC reagent, 5mL distilled water, the Na of 3mL12.5%
2cO
3solution, under 764nm measures its absorbance after reacting 1h under 30 DEG C of water bath condition.
Taking gallic acid concentration as X-axis, the standard curve set up as Y-axis of absorbance, obtaining standard curve equation is Y=0.0128X+0.016, when gallic acid concentration is good linear relationship (R with absorbance within the scope of 10ug/mL-70ug/mL
2=0.9998).
embodiment five: the mensuration of Exocarpium Juglandis Immaturus polyphenol yield
By the sample liquid centrifugal 10min under 4500r/min rotating speed after extracting, accurately pipette 1mL supernatant and carry out 100 dilutions.Accurately pipette again 1mL diluent to color-comparison tube, carry out polyphenol concentration determination according to the method for Specification Curve of Increasing, then calculate the yield of polyphenol in sample.Accounting equation is as follows:
Polyphenol yield (mg/g)=
In accounting equation: C is the mass concentration (ug/mL) of polyphenol in the sample recording according to standard curve; N is extension rate; V is extracting liquid volume (mL); M is sample quality (g).
More than setting forth the embodiment in the present invention, is not that the present invention is done to other formal restriction, and these professional personnel can change equivalent embodiment to the technology contents of above-mentioned elaboration.But as long as not departing from technical solution of the present invention content, according to technical spirit of the present invention, just above example is carried out to simple modification, equivalent variations and remodeling, still belong to the protection domain of the technology of the present invention.
Claims (1)
1. the extracting method of an Exocarpium Juglandis Immaturus polyphenol, it is characterized in that, choosing fresh Semen Juglandis is raw material, adopt machine barking method to obtain Exocarpium Juglandis Immaturus, naturally after drying, pulverizing, cross 40 mesh sieves after blanching, Exocarpium Juglandis Immaturus powder after drying is pulverized and sieved adds pure water by liquid ratio 21:1 (mL:g), be placed in ultrasonic extraction equipment, adopt ultrasound wave assisted extraction technique, ultrasonic power 670W, 57 DEG C of heating-up temperatures, single ultrasonic time 5s, ultrasonic off time 5s, ultrasonic omnidistance time 25min, mixing speed 400r/min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104286034A (en) * | 2014-09-26 | 2015-01-21 | 浙江大学宁波理工学院 | Preparation method of hickory nut epicarp extract |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104286034A (en) * | 2014-09-26 | 2015-01-21 | 浙江大学宁波理工学院 | Preparation method of hickory nut epicarp extract |
| CN105361185A (en) * | 2015-11-12 | 2016-03-02 | 横山县红梦园科技实业有限公司 | Method for separation purification of walnut green seedcase polyphenol substances by macroporous resin |
| CN105920089A (en) * | 2016-04-27 | 2016-09-07 | 云南齐茂盈农农业科技有限公司 | Method for preparing plant total polyphenol from walnut green peel through efficient separation |
| CN105816518A (en) * | 2016-04-29 | 2016-08-03 | 华南农业大学 | Walnut green seedcase phenol natural antioxidant and preparing method and application thereof |
| CN105816518B (en) * | 2016-04-29 | 2020-02-07 | 华南农业大学 | Walnut green seedcase phenol natural antioxidant and preparation method and application thereof |
| CN108499610A (en) * | 2018-04-08 | 2018-09-07 | 江西省科学院应用化学研究所 | A kind of preparation method preparing pucherite@metals-polyphenol complex composite material of core-shell structure using green peel of walnut crude extract |
| CN108499610B (en) * | 2018-04-08 | 2020-09-29 | 江西省科学院应用化学研究所 | Preparation method for preparing bismuth vanadate @ metal-polyphenol complex core-shell structure composite material by using walnut green husk crude extract |
| CN113180220A (en) * | 2021-05-21 | 2021-07-30 | 江南大学 | Pretreatment method of walnut kernels |
| CN113180220B (en) * | 2021-05-21 | 2022-10-11 | 江南大学 | Pretreatment method of walnut kernels |
| CN113499361A (en) * | 2021-07-28 | 2021-10-15 | 西北农林科技大学 | Method for extracting terpenoid substances in walnut green seedcase |
| CN113559146A (en) * | 2021-07-28 | 2021-10-29 | 西北农林科技大学 | Method for efficiently extracting walnut green husk polyphenol substances by electron beam irradiation |
| CN113559146B (en) * | 2021-07-28 | 2022-06-03 | 西北农林科技大学 | Method for efficiently extracting walnut green husk polyphenol substances by electron beam irradiation |
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